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7-Amino-4-methylcoumarin → 2-methyl-3,4-dihydro-4-oxo-N-(2-oxo-4-methyl-2H-1-benzopyran-7-yl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide

HRID 2057888
ノート
印刷プレビュー

反応式

HRID 2057888 の反応式
CO[C:3]([CH:5]1[C:10](=[O:11])[C:9]2[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=2[S:7](=[O:17])(=[O:16])[N:6]1[CH3:18])=[O:4].[CH3:19][C:20]1[C:29]2[C:24](=[CH:25][C:26]([NH2:30])=[CH:27][CH:28]=2)[O:23][C:22](=[O:31])[CH:21]=1>C1(C)C(C)=CC=CC=1>[CH3:18][N:6]1[CH:5]([C:3]([NH:30][C:26]2[CH:27]=[CH:28][C:29]3[C:20]([CH3:19])=[CH:21][C:22](=[O:31])[O:23][C:24]=3[CH:25]=2)=[O:4])[C:10](=[O:11])[C:9]2[CH:12]=[CH:13][CH:14]=[CH:15][C:8]=2[S:7]1(=[O:16])=[O:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 922497-Amino-4-methylcoumarinHCID 120152Methyl 3,4-dihydro-2-methyl-4-oxo-2H-1,2-benzothiazine-3-carboxylate 1,1-dioxide

生成物 1

HCID 132906052-methyl-3,4-dihydro-4-oxo-N-(2-oxo-4-methyl-2H-1-benzopyran-7-yl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
170 °C

実験手順

8.1 g of 2-methyl-3,4-dihydro-4-oxo-2H-1,2-benzothiazine-3-carboxylic acid methyl ester 1,1-dioxide and 5.7 g of 4-methyl-7-amino-coumarin are dissolved in 280 ml of xylene and the solution is heated for 21/2 hours in a bath of 170° C. to distill off the methanol formed during the reaction. The reaction mixture is refluxed for a further 5 hours, cooled, and the precipitate is collected by filtration. The precipitate is digested with 100 ml of 2N-hydrochloric acid at elevated temperature, treated with 100 ml of chloroform and extracted. The residue is collected by suction, washed successively with water, ethanol, methylene chloride and diethyl ether, washed, and dried, affording 2-methyl-3,4-dihydro-4-oxo-N-(2-oxo-4-methyl-2H-1-benzopyran-7-yl)-2H-1,2-benzothiazine-3-carboxamide 1,1-dioxide with a melting point above 285° C.

後処理

  1. distillationto distill off the methanol
  2. customformed during the reaction
  3. temperatureThe reaction mixture is refluxed for a further 5 hours
  4. temperaturecooled
  5. filtrationthe precipitate is collected by filtration
  6. additiontreated with 100 ml of chloroform
  7. extractionextracted
  8. customThe residue is collected by suction
  9. washwashed successively with water, ethanol, methylene chloride and diethyl ether
  10. washwashed
  11. customdried

出典と根拠

ORDレコード
ord-749bf7db5a154a30a095a0bb11e46ad8
出典データセット
uspto-grants-1980_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04213980

反応ノート

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